Determination of Drugs in Blood Samples by High Performance Liquid Chromatography Using On-Line Sample Pretreatment Technique

Theflowdiagramofthison linesample pre treatmentsystemisshowninFig .1.Fig .1　Flowdiagramofon linesamplepretreatmentsystem1.degasunit;2 .pump ;3 .autosampler ;4.on linesampledi lutionbypass;5 .mixer;6.highpressureflowswitchingvalve;7.pretreatmentcolumn ;8.…     

Chromium ion incorporation in the crystal structure of BGO

Comprehensive investigations have been performed by EPR and optical spectroscopy for Bi₃GeO₄ crystals doped with chromium ions. It is demonstrated that the known optical absorption spectrum for chromium ions, specifically, the triplet in the region 600–900 nm has an analog in the EPR spectra — the center with electron spin S = 1. The spectrum is described by the spin-Hamiltonian with the parameters D = 550 G, E = 10 G, g _xx = g _yy = 1.915, g _zz = 1.932. The EPR spectrum is dictated by Cr⁴⁺ incorporation at the germanium sites. Luminescence observed in the region 1.2–1.7 μm is also caused by transitions of Cr⁴⁺ with tetrahedral surroundings to germanium sites. Original Russian Text Copyright ? 2005 N. V. Chernei, V. A. Nadolinnyi, N. V. Ivannikova, V. A. Gusev, I. N. Kupriyanov, V. N. Shlegel, and Ya. V. Vasiliev __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 46, No. 3, pp. 444–450, May–June, 2005.     

Microwave spectrum, centrifugal distortion, dipole moment and conformation of 2-methyl-1,3-dioxane

Microwave spectrum of 2-methyl-1,3-dioxane has been investigated in the frequency range 8–40 GHz. Rotational a-type and c-type transitions with J≤40 have been identified. Rotational constants A = 4658.122(2) MHz, B = 2503.221(1) MHz, C = 1783.950(1) MHz and centrifugal distortion constants for the ground vibrational state have been found. Dipole moment components μ_a = 1.43 ± 0.01 D, μ_c = 1.15±0.01 D and overall dipole moment μ = 1.84±0.02 D have been determined. The data obtained are in accord with the chair conformation of the molecule having equatorial arrangement of the methyl group. Original Russian Text Copyright ? 2006 by A. Kh. Mamleev, R. V. Galeev, L. N. Gunderova, M. G. Faizullin, and A. A. Shapkin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No.2, pp. 373–375, March–April, 2006.     

Spectrophotometric and luminescent analysis of polytetrafluoroethylene treated by γ-irradiation near the melting point

Radiation-modified polytetrafluoroethylene (PTFE) that exhibited intense fluorescence in the visible spectral region was prepared. Radiation modification was performed with ⁶⁰Co γ rays at 330°C, a dose of 0.2 MGy, and an atmospheric air pressure ranging from 10⁻³ to 100 mmHg. The fluorescence and electronic absorption spectra of film (95 μm) specimens irradiated under the given conditions were studied. An important role of molecular oxygen in radiation-chemical processes responsible for the generation and buildup of fluorescing entities was revealed. The spectral characteristics of the four most intense fluorescent centers were determined. It was concluded that polyene systems of π bonds-CF₂-(CF=CF)_n-CF₂-(n=4−11) in the product are responsible for fluorescence. A scheme of radiation-chemical transformation resulting in π-conjugated structures was proposed. Original Russian Text ? S.A. Khatipov, R.N. Nurmukhametov, D.I. Seliverstov, A.M. Sergeev, 2006, published in Vysokomolekulyarnye Soedineniya, Ser. A, 2006, Vol. 48, No. 2, pp. 263–270.     

A Novel Synthesis of Isoxazole Derivatives

Thenitronesareveryimportantinorganicsynthesis.TheyhavebeenwidelyutilizedasintermediatesfromwhichcomPlexheterocyclicornaturalcompoundsanddrugs"'weresynthesisedsuchasisoxazoline3andoxazine4.However,theconversionofnitronetoisoxazolebythermaldecompositionhasnotbeenreported.Inthispaper,wedevelopanewsyntheticmethodofisoxazolesfromheterocyclicnitronesasfollows:wi.-"'rtXfa.H;b.3,4-O-CH2-o-;c.4-CH3O,d.4-Cl;e.2-Brf.2-Cl,g.3,4-coCH3;h.3-ro2;i.4-so2;j.4-CH3Experiment8lAdriedroundbottomflaskundernit…     

Synthesis and structure of a complex of copper(II) bromide with bis(benzotriazol-1-yl)methane

The preparation technique of a complex of copper(II) bromide with bis(benzotriazol-1-yl)methane (L), (Cu₂L₂Br₄)_n, is developed. The compound is studied by single crystal and powder X-ray diffraction and static magnetic susceptibility techniques. According to single crystal XRD data, the complex has a layered structure determined by bidentate bridging coordination of L with N(3) and N(3′) atoms to copper(II). The elementary unit of {Cu₂(μ-Br)₂Br₂} polymer has a binuclear structure. The coordination polyhedron is a trigonal pyramid, and the coordination core is CuN₂Br₃. The temperature dependence of effective magnetic moment is studied within an interval of 2–300 K. The nature of the μ_eff(T) dependence indicates that antiferromagnetic exchange interactions dominate in exchange clusters of the complex with an even number of paramagnetic centers. Original Russian Text Copyright ? 2007 by E. V. Lider, A. S. Potapov, E. V. Peresypkina, A. I. Smolentsev, V. N. Ikorskii, A. I. Khlebnikov, and L. G. Lavrenova __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No.3, pp.543–547, May–June, 2007.     

Complexation of copper(II) with 3-(2-hydroxyphenylazo)pentadione-2,4

It is shown that 3-(2-hydroxyphenylazo)pentadione-2,4 (H₂L) can exist in three tautomeric forms (enol-azo, keto-azo, and hydrazo). The effective atomic charges in the tautomeric forms of H₂L are calculated by the Hückel MO LCAO method. The molar fractions and molar absorptivities of the tautomers at different pH are found. The complexation of copper(II) with H₂L is studied by spectrophotometry. Beer’s law is obeyed for 0.51–5.12 μg/mL of copper. The assumed complex structure is given. The effect of foreign ions and masking agents on the complexation is studied. A procedure for the photometric determination of copper(II) in zinc-based alloys is proposed. Original Russian Text ? S.R. Gadzhieva, T.M. Mursalov, K.T. Makhmudov, F.G. Pashaev, F.M. Chyragov, 2006, published in Zhurnal Analiticheskoi Khimii, 2006, Vol. 61, No. 6, pp. 598–603.     

Phase equilibria and thermodynamic properties of the system Tl-TlCl-Se

Phase equilibria in the system Tl-Se-Cl were studied in the region Tl-TlCl-Se by DTA, X-ray powder diffraction, emf measurements concentration circuits (−) Tl/glycerol + KCl + TlCl/(Tl-Se-Ce) (+), and microhardness measurements. Several vertical sections, an isothermal section at 400 K, and the liquidus-surface projection were constructed. The primary crystallization regions and homogeneity regions of phases were determined, including the α phase of variable composition based on Tl₅Se₂Cl, the only ternary compound of the system. The types and coordinates of invariant and monovariant equilibria on the T-x-y diagram were determined. From the results of emf measurements, the standard thermodynamic functions of formation and the standard entropy were calculated for the compound Tl₅Se₂Cl. Original Russian Text ￠ D.M. Babanly, Yu.A. Yusibov, M.B. Babanly, 2007, published in Zhurnal Neorganicheskoi Khimii, 2007, Vol. 52, No. 5, pp. 819–826.     

国际会议消息

第5屆国际高分子会议(5th SPSJ Infernational Polymer Conference)(IPC94)将于1994年11月28日至12月2日在日本大阪市举行。内容分一般题材;1.聚合物合成与反应,2.聚合物结构与表征;3.聚合物的物理性质;4.聚合物加工;5.功能性聚合物;6.高性能聚合物。选择专题:1.烯烃聚合新进展;2.聚硅烷和含硅聚合物;3.光学活性聚合物;4.生物和与生物有     

《分析试验室》专辑介绍

《国外分析化学述评专辑》(1982年第3辑)编译了近几年发表的15篇文章,涉及分析化学及其基础知识各方面内容。1.检出限和灵敏度;2.现代光学发射光谱分析光源;3.原子吸收光谱分析的共价氢化物发生法;4.化学X射线荧光分析;5.Ar和Ar-H_2电感耦合等离子体作为原子发射光谱分析激光源的严格比较;6.阳极溶出伏安法中第三元素的影响;7.高灵敏度无机分光光度法;8.室温磷光法——一种有前途的痕量分析方法;9.半导体分析;10.金属中气体分析;11.微量待测元素的富集;12.有色金属工业中的ICP发射光谱分析;13.     

Molecular structure of di-<Emphasis Type="Italic">tert</Emphasis>-butylamine-containing the monoedge-functionalized clathrochelate iron(II) <Emphasis Type="Italic">tris</Emphasis>-dioximate

The structure of 1,8-bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza-4,5,11,12-tetraphenyl-17,18-bisc(tert-butylamino)-bicyclo[6.6.6]eicosa-3,5,10,12,16,18-hexaene(2−)iron(2+) tris-dioximate clathrochelate was determined by X-ray diffraction (XRD) analysis. The compound has a molecular structure and crystallizes as triclinic crystals: a = 10.7673(2) Å, b = 11.9520(4) Å, c = 22.5473(7) Å, α = 75.729(1)°, β = 89.161(1)°, γ = 65.334(1)°, V = 2542.64(13) ų, Z = 2, space group 1. P1ˉ. Original Russian Text Copyright ? 2007 by A. B. Burdukov, N. V. Pervukhina, M. A. Vershinin, and Ya. Z. Voloshin __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 366–369, March–April, 2007.     

Synthesis and structure of a new molecular octahedral cluster complex Mo<Subscript>6</Subscript>Se<Subscript>8</Subscript>(Ph<Subscript>3</Subscript>P)<Subscript>6</Subscript>·2H<Subscript>2</Subscript>O

Mo₆Se₈(Ph₃P)₆·2H₂O cluster complex has been synthesized and its structure has been defined. The compound is triclinic, space group P1ˉ, with unit cell parameters a = 14.3356(5) Å, b = 15.7882(4) Å, c = 25.3949(8) Å, = 95.9750(10)°, β = 91.1030(10)°, γ= 112.2570(10)°, V = 5279.8(3) ų, Z = 2, ρ_calc = 1.772 g/cm³. The complex has a molecular structure. The molybdenum atoms of the {Mo₆Se₈} cluster nucleus are coordinated by the phosphorus atoms of triphenylphosphine molecules. Original Russian Text Copyright ? 2007 by Yu. V. Mironov, Zh. S. Kozhomuratova, D. Yu. Naumov, and V. E. Fedorov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 389–393, March–April, 2007.     

Anodic voltammetric behavior of ascorbic acid and its selective determination in pharmaceutical dosage forms and some Rosa species of Turkey

Ascorbic acid is the most common electroactive biological compound found in some plant species (e.g., Citrus species, Rosa species). The electrochemical oxidation of ascorbic acid was investigated by cyclic, linear sweep, differential pulse (DPV), and square wave (SWV) voltammetry. For analytical purposes, a very well-resolved diffusion-controlled voltammetric peak was obtained in acetate buffer at pH 3.50 for DPV and SWV. The linear response was obtained in the range of 3.52–176.1 μg/mL with a detection limit of 0.88 μg/mL for DPV and 0.52 μg/mL for SWV. Based on this study, simple, rapid, selective, and sensitive voltammetric methods were developed for the determination of ascorbic acid in pharmaceutical dosage forms and Rosa species (R. dumalis ssp. boissieri var. boissieri, R. canina, R. pulverulenta, R. heckeliana ssp. vanheurckiana, and R. montana subsp. woronowii). The results obtained are compared with the HPLC data. The developed methods enable the extracts to be analyzed without the necessity of any time-consuming separation. The text was submitted by the authors in English.     

第23届国际光谱学术会于1983年在荷兰阿姆斯特丹召开

第23届国际光谱学术会(包括第10届国际原子光谱学会议)将于1983年6月26日～7月1日在荷兰首都阿姆斯特丹国际会议中心 RAI 召开。会议由“荷兰皇家化学学会”和“分析化学部”主办,L.de Galan 教授为会议主席。包括下列光谱学专题:1.原子发射光谱学;2.原子吸收光谱学;3.原子荧光光谱学;4.X 射线光谱学;5.红外和拉曼光谱学;6.紫外和可见光谱学;7.表面和薄层分析的光谱方法;8.无机分析的质谱法;9.激光光谱;10.检测系统;11.标样     

Ba3 ? xSrxSm(BO3)3 Solid Solutions (0 < x < 3)

Samples of a continuous series of Ba_{3 − x} Sr _x Sm(BO₃)₃ solid solutions (0 < x < 3), crystallizing in the trigonal crystal (system, space group R3ˉ) were synthesized by solid-phase reactions. Formation of a continuous series of solid solutions in the system was confirmed by X-ray phase analysis. The X-ray characteristics of phases of variable composition were determined. __________ Translated from Zhurnal Prikladnoi Khimii, Vol. 78, No. 12, 2005, pp. 2054–2055. Original Russian Text Copyright ? 2005 by Khamaganova, Oshorova.     

Synthesis and crystal and molecular structure of the mixed-ligand coordination compound ZnPhen(n-C4H9OCS2)2

A mixed-ligand complex ZnPhen(n-BuOCS₂)₂ has been synthesized. The structure of the compound was solved by X-ray diffractometry (X8 APEX diffractometer, MoK _α radiation, 4254 F _hkl , R = 0.0448). Triclinic crystals with the parameters a = 9.4464(3) Å, b = 11.0279(4) Å, c = 13.6528(6) Å;α = 106.940(1)°, β = 98.382(1)°, γ = 106.347(1)°; V = 1264.72(8) ų; Z = 2, space group 1. P1ˉ. The structure consists of discrete mononuclear molecules. The polyhedron of the Zn atom is a trigonal bipyramid N₂S₃ formed by coordination of the N atoms of the bidentate Phen molecules and the sulfur atoms of the monodentate and cyclic bidentate xanthate ligands. Dimer assemblies are formed in the structure due to π-π interactions of Phen molecules. Original Russian Text Copyright ? 2006 by R. F. Klevtsova, T. G. Leonova, L. A. Glinskaya, and S. V. Larionov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 47, No. 6, pp. 1189–1194, November–December, 2006.     

加拿大Humphreys教授在北京举行化学教学问题讲座(1985.10)

加拿大Mcmaster大学化学系教授、加拿大化学会教育委员会前主席D.D.Humphreys应邀在北京钢铁学院举行化学教学问题讲座。题目共十个;1.实验的意义;2.课堂演示实验的作用;3.如何教授百人的大班;4.培养解决问题技能的发展;5.不讲课的教学方式和方法;6.如何开设更好的课程;7.选择评定教     

Synthesis of Mn(Ⅲ) Complexes of New "Tailed" Porphyrins and Their Application as Carriers for PVC Membrane SCN-Anion-Selective Electrode

Itiswell~thaboonmemraneelotboonq~anunnitunorPboghulumsaltshavthesamtherselchtympncefClo->SCN>I->Ncy>BrryNo2'>Cl-,~tliisSel~Iy~is~SolelyonthelipopechofthebolIl.~fOr~withthcSe~ty~,whichis~frOmtheboPattenyisthcSUbectOfaSerieSof~.bo,metalloporPbyrinShaVeboeInP~asactiVecomrenentsintheaesignornewpotwlcmoriuerevcmemtrraedon-scltheelot.Insuchcases,the~potendometricboonseltalvityisdependentonthepecnatUrOftheCentralmetalion,withwhichthCse~edailigationedonscanm.Se~tympalsobeaiteredbychangint…     

Conformation changes in the DNA molecule caused by γ-irradiation of its water ethanol solutions of great ionic strength

The conformation changes in DNA in water ethanol solutions (ethanol content 0–22 wt.%, ionic strength μ = 0.15 M NaCl) exposed to γ radiation (10 Gy and 30 Gy doses) were investigated by low-gradient viscosimetry, birefringence in a flow, circular dichroism (CD), and UV spectrophotometry. For μ = 0.15 M, the volume of intact DNA remained constant over the whole range of alcohol concentrations studied in contrast to water alcohol solutions of lower ionic strength, in which the specific volume of the macromolecule decreased cooperatively at a critical concentration of alcohol corresponding to a structure disturbance of water (C _cr = 16.5 wt.% for ethanol). Inversion of the dependence of the specific volume of DNA on the radiation dose, which was found previously for water alcohol solutions with μ = 0.003 M NaCl, vanished under these conditions. For μ = 0.15 M, the dependence of V _sp of DNA on C _eth had no features at C _eth = C _cr; at C _eth ≥ 1.7 wt.% the volume of the macromolecule did not change after irradiation with doses of up to 40 Gy. This is probably explained by the fact that at high salt concentrations the alcohol loses its influence on the structure of the solvent, and its role in the process of γ irradiation is restricted to interception of the active products of water radiolysis. __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 4, pp. 783–788, July–August, 2007. Original Russian Text Copyright ? 2007 by S. V. P ston, I. M. Zyryanova, Yu. V. Zaichikova, and V. V. Zamotin     

Crystal structure of the 1:3 thiourea-hexachloroethane inclusion compound at 295 K

The crystal structure of the 1:3 thiourea-hexachloroethane inclusion compound at 295 K has been determined. The parameters of the rhombohedral Bravais cell (space group R3ˉc) are a = 16.097(2) Å, c = 12.450(3) Å, V = 2793.6(8) ų, d _calc = 1.659 g/cm³, d _exp = 1.661±0.005 g/cm³, Z = 6 for C₅H₁₂Cl₆N₆S₃. The disordered guest molecules lie in the channels (parallel to the c axis) of the clathrate framework constructed from thiourea molecules linked by N-H...S hydrogen bonds. The mutual arrangement of the carbon and chlorine atoms is such that they define four orientations of the C-C bond relative to the channel of the host framework with nearly eclipsed conformations of hexachloroethane: one orientation along the triple bond axis (channel axis) and three equiprobable orientations at an angle of 74(2)° to the axis; for the coaxial orientation, there are two different configurations of the guest with slightly different geometries. The relative contributions of each of the five orientations were determined from the site occupancies of the guest atoms: 26.18 (coaxial orientations) and 3×19%. The resulting structure model is compared with the literature data about guest disordering in the structure of an adduct of the same composition determined at 233 K and with other similar structures. Original Russian Text Copyright ? 2007 by S. F. Solodovnikov, G. N. Chekhova, G. V. Romanenko, N. V. Podberezskaya, Z. A. Solodovnikova, D. V. Pinakov, and A. R. Semenov __________ Translated from Zhurnal Strukturnoi Khimii, Vol. 48, No. 2, pp. 348–357, March–April, 2007.